Method for preparing 2-amino-4-nitrophenol by using disperse blue 2BLN byproduct

A technology for nitrophenol and dinitrophenol is applied in the field of preparing 2-amino-4-nitrophenol, and can solve the problem of low content and purity of 2,4-dinitrophenol, reduction of recycling efficiency, value, pH Poor adjustment and other problems, to achieve the effect of high practical application value, reduce adverse effects, and reduce the trouble of processing

Active Publication Date: 2017-10-17
青岛海湾集团有限公司
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Problems solved by technology

[0012] "Journal of Shenyang University of Technology" in February 1999, Volume 21, No. 1, reported the method of "synthesizing 2-amino-4-nitrophenol with dye waste liquid as raw material", which effectively improved 2-amino-4-nitrophenol The purity of base phenol, but this method is in t...

Method used

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  • Method for preparing 2-amino-4-nitrophenol by using disperse blue 2BLN byproduct
  • Method for preparing 2-amino-4-nitrophenol by using disperse blue 2BLN byproduct
  • Method for preparing 2-amino-4-nitrophenol by using disperse blue 2BLN byproduct

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Embodiment 1

[0060] Utilize the method for preparing 2-amino-4-nitrophenol by-product of disperse blue 2BLN, comprises the following steps:

[0061] A) adjust the pH of the mother liquor in the hydrolysis reaction step in the preparation process of disperse blue 2BLN to be 2.2, and filter to obtain the crude product of 2,4-dinitrophenol;

[0062] B) 35 g of the crude product obtained in step A) is beaten with water, and reduced with sodium hydrosulfide in a buffer system of ammonium chloride (the amount of ammonium chloride is prepared by dissolving 28 g of water), and the reaction temperature is controlled to be 85° C.;

[0063] C) Control the reaction end point of step B) by liquid chromatography, add sodium chloride for salting out after the end point is reached, cool to 5° C. and filter to obtain the crude product of 2-amino-4-nitrophenol;

[0064] D) dissolving the crude product obtained in step C) in water, raising the temperature to 81° C. and filtering while hot;

[0065] E) Acidi...

Embodiment 2

[0069] Utilize the method for preparing 2-amino-4-nitrophenol by-product of disperse blue 2BLN, comprises the following steps:

[0070] A) adjust the pH of the mother liquor in the hydrolysis reaction step in the preparation process of disperse blue 2BLN to be 3.0, and filter to obtain the crude product of 2,4-dinitrophenol;

[0071] B) 30 g of the crude product obtained in step A) is beaten with water, and reduced with sodium hydrosulfide in a buffer system of ammonium chloride (the amount of ammonium chloride is prepared by dissolving 7.5 g in water), and the reaction temperature is controlled to be 55° C. ;

[0072] C) Use liquid chromatography to control the reaction end point of step B), add sodium chloride to salt out after the end point is reached, cool to 8°C, and filter to obtain the crude product of 2-amino-4-nitrophenol;

[0073] D) dissolving the crude product obtained in step C) in water, raising the temperature to 65° C., and filtering while hot;

[0074] E) Ac...

Embodiment 3

[0078] Utilize the method for preparing 2-amino-4-nitrophenol by-product of disperse blue 2BLN, comprises the following steps:

[0079] A) adjust the pH of the mother liquor in the hydrolysis reaction step in the preparation process of disperse blue 2BLN to be 2.5, and filter to obtain the crude product of 2,4-dinitrophenol;

[0080] B) 18.5g of the crude product obtained in step A) is beaten with water, reduced with sodium hydrosulfide in the buffer system of ammonium chloride (the consumption of ammonium chloride is prepared by dissolving 5.55g in water), and the control reaction temperature is 60 ℃;

[0081] C) Control the reaction end point of step B) by liquid chromatography, add sodium chloride for salting out after the end point is reached, cool to 25° C. and filter to obtain the crude product of 2-amino-4-nitrophenol;

[0082] D) dissolving the crude product obtained in step C) in water, raising the temperature to 70° C. and filtering while hot;

[0083] E) Acidify t...

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Abstract

The invention belongs to the technical field of chemical industry, and more specifically relates to a method for preparing 2-amino-4-nitrophenol by using a disperse blue 2BLN byproduct. The method comprises the following steps: A) adjusting the pH value of mother liquor in a hydrolysis reaction step during a disperse blue 2BLN preparation process to 2.2-3.0, filtering the material to obtain a 2,4-dinitro phenol crude product; B) adding water in the crude product obtained in the step A) for beating, using sodium sulfhydrate for reduction in an ammonium chloride buffer system; C) using liquid chromatogram for controlling a reaction terminal point of the step B), adding sodium chloride for salting-out after arriving the terminal point, cooling the material and filtering the material to obtain a 2-amino-4-nitrophenol crude product; D) dissolving the crude product in the step C) in water, heating the material and filtering the material while hot; E) acidifying the crude product, cooling the material and performing suction filtration on the material, and washing the material; and F) drying a filter cake.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing 2-amino-4-nitrophenol by using disperse blue 2BLN by-products. Background technique [0002] In the process of preparing disperse blue 2BLN, the mother liquor produced by the hydrolysis reaction process contains a large amount of by-product 2,4-dinitrophenol, and the main chemical reaction equation of this by-product is as follows: [0003] [0004] This substance is directly used as a by-product with low purity and bad color state, so it cannot be used. If the by-product is treated as waste water, a large amount of 2,4-dinitrophenol is wasted; in addition, because the mother liquor has high chroma, high Chemical oxygen demand and other characteristics, the processing procedure is complicated, the cost of recycling is high, and the purity of 2,4-dinitrophenol recovered by the existing method is low, it is difficult to meet the needs...

Claims

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Application Information

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IPC IPC(8): C07C215/76C07C213/00C07C213/10
CPCC07C201/16C07C213/00C07C213/02C07C213/10C07C215/76C07C205/23
Inventor 张英民李广顺马在河王蒙刘方先韩建朝张美艳全健
Owner 青岛海湾集团有限公司
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